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The hexaethylcyclohexaarsoxane complexes [{M(CO) 3 } 2 {cyclo-(C 2 H 5 AsO) 6 }], M = Cr, Mo, W, 2-4 have been prepared by the reaction of (C 2 H 5 AsO) n  with the respective metal hexacarbonyl in toluene and characterized by their IR and NMR spectroscopic data. For 2 the molecular structure was established by X-ray structural analysis. The 12 atoms of the As 6 O 6  ring form a flattened cuboctahedron in which the 6 oxygen atoms lie in the central equatorial plane. Cr(CO) 3  groups are coordinated facially by the upper and lower three arsenic atoms. An approximately S 6  symmetry is displayed by the Cr 2 As 6 O 6  core. Average values of respectively 116.3 and 98.9° are observed for the As–O–As and O–As–O angles in the hexadentate ligand. The ΕΙ-MS and  1 H NMR data for (C 2 H 5 AsO) n  suggest that this alkylcycloarsoxane is present in solution as a mixture of species including trimers and tetramers so that a metal assisted ring expansion is required for the formation of 2-4.

Synthesis and Structure of the Hexaethylcyclohexaarsoxane Complexes [ { M(CO) 3 } 2 {cyclo-(C 2 H 5 AsO) 6 }], M = Cr, Mo, W